Operation of pressure stills



Dec. 31, 1929. J, BELL OPERATION oF PRESSURE STILLs 2 Sheets-Sheet 2 Filed March 24, 1924 INVENTOR ATroNEYs .Patented Dec. 3l, 1929 j `ally condensing the vapors from pressure JOHN E. `BELL, 'OF BROOKLYN, NEW' YORK, ASSIGNOR T0 SINCLAIR REFINING COM- PANY, F CHICAGO, ILLINOIS, A CORPORATION OF MAINE OPERATION OF PRESSURE STILLS Application 1ed March 24, 1924. Serial No. 701,397.

, This invention relates to an improved method of operating 'pressure stills and 1nvolves an improved method of tractionstills whereby accurate fractionation is obtained directly.

The invention relates particularly to nnprovements in the operationot' tractionating towers employed in conjunction with pressure stills having reflux towers thereon, tor

- cracking hydrocarbon oils of higher boiling point such as gas oils and the like to form more volatile or lighter hydrocarbon oils such as those which constitute commercial gasoline or pressure distillate.

In cracking hydrocarbon oils by distillation under pressure, the crude 'pressure distillate discharged from the top of the reliux tower through which the vapors are passed from the pressure still may contain, in addition to the lighter hydrocarbons suitable as components of gasoline, hydrocarbons ot the kerosene group and others even heavier. lt has heretofore been customary to subject all of the vapors from the reux tower on the pressure still to condensation in a connnon receptacle and to fractionate the condensate so obtained to merchantable products and to separate out the heavier hydrocarbons `by redistillat-ion.

,One of the objects ot the present invention is to partially or entirely dispense with this redistillationby fraction-ally condensing the vaporsv as they come from the reflux tower on the pressure still, separating the heavier components from the lighter components and separately condensing them.

According to this invention, the vapors from the reflux tower on the pressure still are passed successively through a series of separate vapor condensing chambers maintained at progressively lower temperatures and a regulated part of the condensate from condensing chambers at lower temperature is refluxed into condensing chambers of higher temperature. The condensing surfaces in the successive chambers are maintained at progressively lower temperatures so that the heaviest vapors are condensed in the first chamber entered bythe vapors, the next heaviestvapors inl the next chambers entered and so on. By refluxing a part of the condensate from condensing chambers at lower temperature into condensing chambers at higher temperature, the retluxed condensate assists in electing condensation and is subjected to refractionation; and, by regulation of the amount of condensate so reliuxed, the fractional condensation in the condensing chambers into which the reluxed condensate is introduced is controlled.

According to this invention, the accuracy of the fractionation is further promoted by maintaining a low temperature differential between the condensing surfaces and the vapors undergoing condensation thereon. As the temperature ot' thecondensing surface approaches the critical temperature of the vapor to be condensed the more accurate is the fractionation, and it is desirable, for close fractionation` that the condensing surfaces be maintained at temperatures just below the critical temperatures ot' the respective vapors to be condensed. Practically,

however, it is necessary to sacrifice, to a certain ext-ent, accuracy or deiiniteness in cut because of the large number ot compounds of dilterent gravity in the vapors to be condensed and the increased extent of condensing surface necessary where a lower temperature differential is maintained.

ln carrying out the improved process of the present invention, it is advantageous to maintain a differential of less than about 25 F. between the temperature of the cooling fluid circulating over the condensing surfaces and the ten'iperattue of the vapors undergoing condensation thereon, the temperature of the condensing surface being somewhere intermediate-the temperatures of the cooling medium and the vapors respectively. The temperature differential of EVO F. between the cooling medium entering each condensing chamber and the vapors leaving the same chamber is substantially maintained throughout the condensing chambers of the series. The temperature differential may be lower, say ll)o F. -for example, with corresponding increase in the size of the apparatus if the same number and character of v 25 mainly revaporized in a hotter chamber,

cuts'are to'be made. For example, to condense all of the vapors lfrom the reflux tower on the pressure still in the fractional con- Y denser, including the gasoline` fraction, with 5 a temperature differential-of 25o FJ, assuming the vapors from therefluxtower on the pressure `still have a temperature of about 530 F. when they'reach the fractional condenser, thecooling medium for cooling and 10 condensing thevapors' would enter at a temperature of about 65 F. and leave at a temperature of about 505 F. By increasing the flow'of the cooling medium, or by decreasing its initial temperature, greater condensation can be achieved, but vat the expense of the accuracy of the cuts obtained.

' According tothe present invention,l a regulated part ofthe condensate from condensing chambers at'lower temperature is refluxed into the condensing chambers of next.

higher temperature to increase theeiciency of separation and to control the fractional v condensation.v The condensate'refluxe'd from a ycooler chamber to a hotter *chamber is only a small fraction of heavy com onents which have been carried over with t e' lighter -vapors remaining behind in`liquid form in the` hotter chamber. The reliuxed condensate is lac thus subj ectedtorefractionation and condensation, within the chamber into which lthe yrefluxed condensate is introduced in regu- .lated amount, is controlled by the cooling YeHect of the introduced liquid. condensate '3a and the vaporization thereof. Y Allor a part of the condensate fromv certain of the chambers may be reintroduced into the preceding chamber yat hi her; temperature, and, in some cases,it may .be desirable to by-pass a part' '40 :of the refluxed condensate aboutl the nex't preceding chamber-and 'introduce it into the succeeding chamberat still higher tempera- 'turei 1 condensed may bearranged in vertically superposed positionl in the form of a tower,

the vapors undergoingv fractional condensation entering at the bottom of theftower and leaving from thetopfithereof. The condensing surfaces preferably constitute tubes disposed within thecondensing chambers and through which the cooling fluid flows'. Any\ j. cooling luid, stable at Athe` temperatures to o which it is subjected, may -beemployed, but I find it advantageous to yuse asui'table oil, and to constantly recirculate/it' through the tower counterlcurrent-,tol the flow of vapors. therethrough, through a cooler to absorb theheat from theoil, and back to the tower by means of a suitable pump. That regulated part of the .condensate relu'xed from each of the superposed chambers to the chamber at 66 next higher'temperature may be -returned A The series of separate condensing charn-Y 45 bers. in which the lvapors are fract-ionally.

by gravity to the next lower condensing section 1n the tower.

The invention will be further described in i connection with a pressure still of the general type described and illustrated -injPatent 4N o. 1,285,200 granted vto the Sinclair Refining Company, November19, 1918, on lthe a plication of Edward .W. ,Isom but it wil be understood that the invention is of general application to' the lfractionation. of the vapors discharged from reflux towers on pres-` sure stills. v

In the accompanying j drawings, I have shown certain-forms of apparatus in whichthe process -oflthe invention can be practised andthe invention will be further described inconnection therewith: It is to'be underjstood, however, that these specific illustrations and description are for the vpurpose of exemplification and that the scope ofthe in ventionis defined in the in which lI have endeavored to'distinguish it from the prior art, without, however relinquishing or abandoning ture' thereof. j. In the accompanying'drawings,

Fig. 1 is a fragmentar axial, longitudifollowing claims,

any portion br yfeanal, sectional View of aI ractionating tower vadaped for the practiceof the process of the invention, and- 1 s Fig. 2 represents inelevation and partly i in section a fractionating tower of the type shown in Fig. 1 in conjunction with a pres- L sure still having a reflux tower thereon..

Each part is identified bythe same reference character wherever it occurs in the separate figures.

Referring ating condensing tower comprises a cylin-k drical shell yl closed by end plates) 5, each of which is provided with a hand-hole fitting 6.

The hand-holes are normally closed by plates and 8: Slightly spaced` from the end plate 5 at each end of the tower are header sheets, s' '9 and 10, said sheets v'forming with the adjacent end platesinlet and outlet 11 and 12, for\'the cooling fluid as will presentlyv appear. he ,space between the-header sheets is divided into a plurality ofjv'apor condensing chambers 13, shown as four in number nalthough the number may be varied and is dependent upon the number of cuts desired. Between adjacent vapor condensto the drawings, lthe lfractioni ing chambers are chambers 14 forthe cooly Y y no chambers, 1

.tion for the vapors therethrough in order -the upper vapor condensing chamber to which it is connected is sufficiently above the header sheets forming the bottom of that chamber to allow for the collection of liquid condensate therein.

lVhere oil is employed as the cooling fluid, it is preferably circulated downwardly through the tower and drawn off through the bottoni, cooled, and returned to the top of the tower. For this purpose, the cooling oil may be circulated through an external cooler of the usual tubular construction by means of a circulating pump. The oil may he cooled in this external coolerl by water or other appropriate cooling fluid. In order to supplement the control of the gravitics of the several cuts effected in the respective vapor condensing chambers by regulated refluxing of the condensate separately collected in each chamber, moreror less of the cooling fluid may be by-passed around any of the condensing chambers except the first or it may be carried from any of the cooling fluid chambers directly to the cooler through pipe 32 and the valved connections thereto comvmunicating with the cooling fluid compartments in the tower. Thermometer wells 35 are provided in the connections 2() 4'for observation of the temperature in each of the vapor connections.

Each condensing chamber near its bottom and below the level of the vapor connection thereto, has a draw-off pipe 23, which is provided at 36 with a' gauge glass toindicate the level of the condensate'in the chamber, and a valve 37 for shutting 0H the draw-off and controlling the passage of condensate therethrough. A pipe 38 connected to the gauge glass receptacle extends to a cooler or storage tank. A branch connection 39 leads from the draw-off 23 of each condensing chamber, except the lowermost, to the top of the next lower condensing chamber at 40, a trap being formed in said pipe at 41 and a valve located therein at 42. A regulated part of the condensate from each condensing chamber is refluxed through this connection to the next lower and hotter condensing chamber where it is revaporized and returned for further treatment, the amount of'reflux so introduced into the next lower and hotter chamber being controlled by valve 42. The stream of condensate entering the top of condensing chamber from pipe 39 s reads over the topmost baille therein, and, tie holes in the baffle through which the cooling tubes extend being somewhat larger than the latter,forms films on the tubes until vaporized, being thus effectively subjected to the temperature 'of the tubes. .The refluxed condensate is thus in effect redistilled and refractionated securing a. more definite eut while at the same time effecting a regu-lated condensation of the vapors of the chamber into which it is introduced.

The pressure still illustrated in Fig. 2 is made up of the bulk supply tank 43 located 80 away from the heating furnace 44, the verF tical heating tubes 45 arranged in the heating flow. 46 of the furnace.and circulating pipes 47, 48 upper ends of the vertical tubes, respectively,

with the bulk s upply tank and a.circulating i pump 50 for circulating the oil from the bulk supply tank through the vertical tubes and back to the bulk supply tank. Arranged 90 above the bulk supply tank is the reflux tower 5l having a series of baffles therein and connected with the vapor dome of the bulk sup-f -ply tank through the vapor line 52. An overflow refluxline 53 leads back to the bulk 95 supply tank. l, The vapors from the top of the reflux tower escape through the vapor line 54 to the` fractionating tower 55 where the vapors from the reflux tower undergo fractional condensation. upwardly through the fractionating tower 55, undergoing fractional condensation during passage, and any uncondensed vapors and gases escape from the top of the tower through connection 56. The vapors escaping 105 through connection 56 may be conducted through a separate condenser, or where they contain no valuable condensible material, may be conducted to a ga's holder, or may be otherwise disposed of. A feed line 61 is provided 110 for feeding fresh oil tothe top of the reflux tower 5l. An additional feed line 62 is provided for feeding oil to the bearings of the pump 50. 'A continuous tar draw-off 1s shown at 57 and a pumping-out line for dis- 115 charging the still is shown at`58.

The pressure may be regulated and reduced by meansy of a regulating valve 59I be tween the reflux tower and the fractionating tower or by the valve 60 r fractionating tower. .The fractional coni densation of the vaporsfrom the refluxetower passing through the fractionating tower. 55 may be effected under the pressure prevailing in the still system, sation of the vapors from the refluxt'ower may be effected at atmospheric pressure or other suitable intermediate or reduced pres- SuIe.

The fractionating tower 55 is of the con- 130 and 49 connecting the lower and 85 The vapors pass located beyond `the V.120

or the fractional eenden s truction shown -in somewhat more detail in Fig. 1, and is provided with four vapor condensingchambers. The cooling fluid, at a`ppropriate temperature, is introduced finto the upper cooling fluid compartment tower through connection 2 8, passed downwardly through-the cooling tube andintermedate cooling compartments in the tower, and re- Omoved 'through connection 25. .The hot temperature,

collected in the lower -in the lowermost `and hottest chamber 13,

the next heaviest vapors in the next chamber 13b and the progressively lighter fractions in the successive chambers 13c and 13d, the condensate in each chamber being separately part lof that` chamber. The liquid condensate collecting in the lowermost chamber 13", is Withdrawn through connection 23. A regulated partof the condensate' collecting -in each ofthe chambers,

13b, .13 and 13d, may be refluxed into the.

next lower and next hotter chamber through Controlled in each the connections 41"'V 4 1b and 41c respectively, the amount of condensate so returned being 42 respectively. That part of Athe condensate collecting in each of these upper chambers whlch is not reiuxed into'the preceding chamber is withdrawn through the receptacles 36.

Incarrying out the'process of the inven- I tion, yin con3unction with the--pressurerdistill ation of relatively heavy hydrocarbon oils Yfor the production of gasoline, the heavier vapors are condensed in the reflux tower 51 by -heat exchange with the fresh feed introl vduced'through connection 61 and returned condensed in the the fractionating to the still through connection 53. The vapors escaping from the reflux tower through connection 54 comprise the gasoline component, kerosene character fractions, and some heavier vapors. Theagasoline fraction, toget'her -with the lfractionating tower 55, or' tower 55 maybe so operated` as to separate the heavier components from t f fraction s 6o.

e gasoline fraction and the gasoline may be conducted to' a separate condensers through connection 56. Where theA gasoline tio'nating tower,

'fraction is condensed. in the fracthe gasoline may be condensed in the uppertwochambers and the kerosene and heavienfractions condensed in the two lower chambers. Where'the gasoline condensing chamber. The un-A case by valves 42a, 421 and heavier fractions, may bel fraction is separately condensed, the heavierA in the chambers of the fractionating tower, for example, kerosene character fractions may be collected in the upper-three chambers anda heavier fraction in the lower chamber. The fractions condensed in the chambers of the tower may be marketedas such, or after further refining treatment, or the different fractions may be blended with each other or withy other stock "in a variety of ways according tothe specific composition desired.v If no kerosene'is desired, the tower may be operated with a smaller drop in temperature of the cooling medium in the tower.

The heavier fraction condensed in the lowermost and hottest chamber 13a may be returned to the still .directly through connections 23 and 63.. Such of the other fractions as may be desired may likewise be returned to the still throughthe valved connections communicating between the connection 63 and the receptacles 36. Where the fractionating tower is operated at a lower pressure than that prevailing in the still fractions may be separated into various cuts...

system, the fractions` returned to the still through connectionv 63 are forced into the still circulating connection 48 through pipe 64 by means of pump 65. Excess oil over that amount required for introduction into the still may be ,conducted to suitable storage receptacles through connection 66.

It would be apparent that, in one aspect,

this invention provides anoperation, which,

substituted for the customary final condensation of the vapors discharged from the reflux tower on a pressure still, effects a separation of the vapors into the vdesired' fractions directly as they come from the .pressure still, without redistillation. It will further be seen that this invention provides an improved method of fractionating and condensing vapors from a pressure still whereby they aredivided into definite cuts or fractions whichare under the operators control. One

of the important advantages of the invention is the elimination of the redistillation of crude pressure distillate.

I claim: I 1. The improvement in the operation of `pressure stills which comprises heating the oil under pressure at a cracking temperature, passing the vapors generated thereby through a path of restricted cross-section to a separate refluxing zona-'controlling the refiuxin'g operation in saidseparate refiuxing zone by passing fresh feed oil for the still in direct Contact with and countercurrent to the flow of vapors therein, passing the remaining vapors through a series of condensing chambers maintained at progressively' lower temperatures, cooling the vapors inv said condensing chambers by passing a cooling Huid having atemperature only slightly Y fluxing operation in said Veo from the first named iefiuxing operation to the pressure still.

2. The improvement in the operation of pressure stills which comprises heating the oil under pressure at a cracking temperature, passing the vapors generated thereby through a path of restricted cross-section to a separate refluxing Zone, controlling the reseparate refluxing Zone by passing fresh feed oil for the still in direct contact with and countercurrent to the flow of vapors therein, passing the remaining vapors through a series of condensing chambers maintained at progressively lower temperatures, cooling the vapors in said condensing chambers by passing a cooling fluid having a temperature only slightly lower than that of the vapors being cooled in indirect heat exchanging relation with the vapors in said condensing chambers, controlling the condensation in the said condensing chambers of higher temperature by returning -in part the reflux condensate fromcondensing chambers of lower temperatures, and returning reflux condensate from. at least one of said condensing chambers directly to a point in the still where it will pass immediately through the heating zone.

3. The improvement in the operation of pressure stills which comprises heating the \oil` under pressure at a cracking temperature,

passing through a path of restricted cross-section to the vapors generated thereby a separate refluxing zone, controlling the reflux operation in said. separate refluxing zone by passing fresh feed oil for'the still in direct contact with and countercurrent to the flow of yapors therein, passing the remaining vapors through a series of condensing vchambers maintained at progressively lower temperatures, cooling the vapors in said'condensing chambers by passing a cooling fluid having a temperature only slightly lower than that of the vapors being cooled in indirect heat exchanging relations with the vapors in said condensing chambers, controlling the condensation in the said condens- Wing chambers of higher temperature by returning in part the reflux condensate from condensing chambers of lower temperatures, and returning reflux condensate admixed with fresh oil from the first named refluxing operation to the pressure still.

4. The improvement inthe operation of pressure stills which comprises heating the oil under pressure at a cracking temperature,

passing the vapors generated thereby through a path of restricted cross-section tom, i

a separate refluxing zone and controlling the refluxing operation in said separate refluxing zone by passing fresh feed oil for the still in direct Contact with and countercurrent to the flow of vapors therein, reducing the pressure on the .remaining vapors and passing the vapors under reduced pressure through a condensing chamber, cooling the vapors in said condensing chamber by passing a cooling fluid having a temperature only slightly lower than that of the vapors being cooled in indirect heat exchanging relation with the vapors in said condensing chamber, passing the vapors still uncondensed through a separate condensing chamber at a lower temperature, separately collecting the condensate in each condensing chamber and controlling the condensation in the first chamber by returning in part the reflux condensate from the second chamber to the first chamber, and returning reflux condensate admixed with fresh oil from the first named refluxing operation tothe pressure still.

5. The improvement in the operation of pressure stills which comprises heating the oil under pressure at a cracking temperature, passing the vapors generated thereby through a path of restricted cross-section to a separate refluxing zone, controlling the refluxing operation in said separate refluxing zone by passing fresh feed oil for the still in direct Contact with and countercurrent to the flow of vapors therein, passing the remaining vapors through a series of condensing chambers maintained at progressively lower temperatures, cooling the vapors insaid condensing chambers by passing a cool1ng fluid having a temperature only. slightly lower than that of theivapors being cpoled in indirect heat exchanging relation with the vapors in said condensing chambers, separately collecting the condensate in said condensing chambers, controlling the condensation in the said condensing chambers of higher temperature by returning in part the reflux condensate from said condensing chambers of lower temperatures, and returning at least one of the heavier condensates to the pressure still.

6. The improvement in the operation of pressure stills which comprises heating the oil under pressure at a cracking temperature, passing the vapors generated thereby through a path of restricted cross-section to aseparate refluxing zone, controlling the refluxing operation in said separate refluxing zoneby pass-y temperature only slightly lower than that of controlling the Ythe vapors being cooled inindirect heat ex-.

changing relation with t-he vaporsin said condensing chambers and returning reflux condensate ,'from the 1 condensing chamber. of

highest temperature to the pressure still.y l -V The improvement in the operation of l pressure stills forcrackinghydi'ocarbon oils ,.-to produce gasoline, whichS comprises heating the oil under pressure at a cracking temperature, passing the vapors generated thereby through a path of restricted cross-section to a `separate reuxing luxing operation in zone by passing freshfeed oil for the still in direct Contact with and countercurrent to the flow of vvapors therein, passingv the remaining vapors througha 'separate condensing chamber, cooling the vapors in said condensing chamber by passinga cooling luidrhaving a temperature onlyslightly lowerlthan that t of the vapors being cooled in indirect heat exireiluxing zone, keration in said changing relation with the vapors therein,4

passing the vapors still uncondensed through a 'separate condensing chamberof lower tem- '25 'parat-ure, 'separately collecting the reflux condensatein each of said c ondensingchambers,

Icondensation in the condensing chamber of higher temperatureby returning in part the .reflux condensate from the said- Mcondensing chamber of lower. temperature, separately condensing the gasoline fraction and separately withdrawing tion heavier than gasoline from said condensing'chambers.

5 8. vThe improvement in 'the' operation of pressure stills which nomprise's Iheating the oil under pressure at a cracking emperature,

passing the vapors generated thereby through a path of restricted crosssection to a separate 4o reiguxing zone, controlling the reluxing operation in said separate refluxing zone by passafing freshl feed oil for the still in with and countercurrentto the therein,

46 through .a series maintained at tures, cooling t chambers-by passing a cooling iuidfhaving a temperature only slightly lower than that of id the vapors being cooled in, indirect heat exy changing relation -with the vapors in said condensingl chambers, and ret.` rnin densate -admixedwith fresh oil om the iirst named refluxing operation to the pressure I5 'still. y

9. The 'improvement-in the o eration of pressure stills which' comprises eating the oil u nder pressure at a cracking temperature, passing the-vapors generated thereby through w apath of restricted crosssction to a separate refluxlng zone, controlling the refluxing op- ,'eration'in said separatehrefluxin'g zone by passing vfresh. feed oil for the still in direct lslight-ly lower than' that of the zone, lcontrolling the re-` said separate refluxing,`

at least one trac'-l direct contact flow of vaporsv passing (the remaining vapors of condensing chambers progressively lower tempera- 'l y] e vaporsin sai-d-condensing.7

through a condensingchamber, cooling the vapors in said condensing chamber by passing a cooling fluid having a temperature only vapors/being cooled in indirect heat exchanging relation vwith the vapors in said condensing chamber,

passing .the vapors still uncondensed to a separate condensing chamber at a lower temperacondensate in 'each condensing chamber. and controlling the wcondensation in the first chamber byv returnture, separately collecting the ing in part the reflux condensate from the sec-' ond chamber tothe first chamber; and returningrelux condensate admixed with fresh oil from the first-named refluxing operationto the pressure st-ill.

10, The improvement -in the operation of pressure stills which comprises heating theA oil under pressure at a crackingtemperature, passing the vapors generated thereby through a path of restricted cross-section to a separate controlling the refluxing opseparate'reflux'ing zone by introducing fresh oil directlyinto direct and intimate contact with the vapors therein, passing the .remaining vapors l ries of condensing chambers maintained at progressively lower temperatures,

vapors in said condensing chambers by passing a cooling .slightly lowt,

fluid having a temperature only thanthat of .the vapors beingA rect heat 'exchanging relation with the -vapors'in said condensing chanfoers, controlling the condensation in said condensing 'chambers of higher temperature by returning in'partfthe reflux condensate from condensing 'chambers of lower temperatures, and returning reiiux condensate admixed with fresh oil-from the first-named retluxing operation tothe pressure still. y

cooled in in Y. In testimony .whereof reflux cont contact 'withand countercurrent to the flowv of It vapors therein., `passing the remaining vapors through a secooling the vr I'aiiix my signature. v JOHN E. BELL.

loo l iis 

